CN105115943A - Gold seed growth based preparation method of terminal reflective optical fiber surface plasmon resonance sensor - Google Patents
Gold seed growth based preparation method of terminal reflective optical fiber surface plasmon resonance sensor Download PDFInfo
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- 239000013307 optical fiber Substances 0.000 title claims abstract description 65
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 239000010931 gold Substances 0.000 title claims abstract description 41
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Abstract
本发明涉及一种基于金种生长的终端反射式光纤表面等离子共振传感器制备方法。裸光纤经氨丙基三甲氧基硅烷处理后，其表面被-NH2功能化；通过与金种的静电相互作用，将金种吸附于裸光纤表面；镀膜液中，金种快速生长为致密的金膜；端面封银后，制得光纤SPR传感器。本发明方法不使用大型且昂贵的镀膜设备，解决了物理镀膜中必须使用转动装置以保证光纤柱面膜厚均匀的缺陷，且制备的传感器对周围环境具有高的灵敏度，分别在折射率为1.333-1.359与1.359-1.386范围内，灵敏度为2054nm/RIU与3980nm/RIU，也可以用来制备棱镜型SPR传感器、各种传输模式及形状的SPR传感器及其它金膜传感器。
The invention relates to a method for preparing a terminal reflective optical fiber surface plasmon resonance sensor based on gold seed growth. After the bare fiber is treated with aminopropyltrimethoxysilane, its surface is functionalized by -NH2 ; through the electrostatic interaction with the gold species, the gold species are adsorbed on the surface of the bare fiber; in the coating solution, the gold species grow rapidly into a dense The gold film; after the end face is sealed with silver, the optical fiber SPR sensor is made. The method of the present invention does not use large and expensive coating equipment, and solves the defect that a rotating device must be used in the physical coating to ensure that the thickness of the optical fiber cylindrical film is uniform, and the prepared sensor has high sensitivity to the surrounding environment, and the sensor has a refractive index of 1.333- Within the range of 1.359 and 1.359-1.386, the sensitivity is 2054nm/RIU and 3980nm/RIU, and can also be used to prepare prism-type SPR sensors, SPR sensors of various transmission modes and shapes, and other gold film sensors.
Description
技术领域technical field
本发明涉及一种基于金种生长的终端反射式光纤表面等离子共振传感器制备方法，属于表面等离子共振谱仪传感器制备方法。The invention relates to a method for preparing a terminal reflective optical fiber surface plasmon resonance sensor based on gold seed growth, which belongs to a method for preparing a surface plasmon resonance spectrometer sensor.
背景技术Background technique
光纤型表面等离子共振(Surfaceplasmonresonance，SPR)传感器，用于监测分子相互作与目标分子定量检测，已广泛应用于疾病诊断、DNA杂交与细胞行为监测、环境与食品安全检测等领域。它不但保持了传统棱镜型SPR传感器高灵敏度、无标记实时检测等特点，并且具有其独特优势，包括：小型化、可抵抗电磁波干扰、可实现远距离传感等。Fiber-optic surface plasmon resonance (SPR) sensors are used to monitor molecular interactions and quantitative detection of target molecules. They have been widely used in disease diagnosis, DNA hybridization and cell behavior monitoring, environmental and food safety testing and other fields. It not only maintains the characteristics of traditional prism-type SPR sensors such as high sensitivity and real-time detection without marking, but also has its unique advantages, including: miniaturization, resistance to electromagnetic wave interference, and long-distance sensing.
均匀的金属膜是SPR传感器拥有高灵敏度、优良的SPR信号的关键。传统的制备光纤SPR传感器方法是使用昂贵的镀膜设备，通过物理蒸发或溅射方法，在光纤上首先镀2-3nm的Cr提高粘附性，再镀45-50nm的贵金属提供自由电子。然而，针对光纤是一个柱面，而不是玻璃片平面的情况，在这些物理镀膜方法中，需要采用复杂的转动装置来保证光纤柱面上金膜的均一性。金种生长的光纤SPR制备方法，不用使用此复杂的转动装置，并且其成本低廉、易于操作，在光纤SPR传感器制备中具有优良的应用前景。A uniform metal film is the key to the high sensitivity and excellent SPR signal of the SPR sensor. The traditional method of preparing optical fiber SPR sensor is to use expensive coating equipment to first plate 2-3nm Cr on the optical fiber to improve adhesion, and then plate 45-50nm noble metal to provide free electrons by physical evaporation or sputtering. However, for the case where the optical fiber is a cylinder instead of a flat glass plate, in these physical coating methods, complex rotating devices are required to ensure the uniformity of the gold film on the fiber cylinder. The optical fiber SPR preparation method of gold seed growth does not need to use this complicated rotating device, and it is low in cost and easy to operate, and has excellent application prospects in the preparation of optical fiber SPR sensors.
发明内容Contents of the invention
本发明目的在于提供一种基于金种生长的终端反射式光纤SPR传感器制备方法。该制备方法操作简单、成本低廉，制备的传感器灵敏度高、稳定性好。本发明是通过以下技术方案加以实现的。The purpose of the present invention is to provide a method for preparing a terminal reflective optical fiber SPR sensor based on gold seed growth. The preparation method has simple operation and low cost, and the prepared sensor has high sensitivity and good stability. The present invention is achieved through the following technical solutions.
本发明的一种基于金种生长的终端反射式光纤SPR传感器制备方法，包括以下步骤：A kind of terminal reflective optical fiber SPR sensor preparation method based on gold seed growth of the present invention comprises the following steps:
a)光纤预处理：将光纤截取小段，光纤小段终端作为传感区域；传感区域浸泡于浓硫酸中，去除光纤表面聚合物；去离子水清洗后，去除聚合物的传感区域浸泡于40％HF中30min，去除光纤包覆层；a) Optical fiber pretreatment: the optical fiber is cut into small sections, and the end of the small section of optical fiber is used as the sensing area; the sensing area is soaked in concentrated sulfuric acid to remove the polymer on the surface of the optical fiber; after cleaning with deionized water, the sensing area where the polymer is removed is soaked in 40 In %HF for 30min, remove the fiber coating;
b)功能化修饰：将步骤a)中获得的光纤传感区域浸泡于食人鱼洗液，光纤表面被-OH修饰后取出，用去离子水清洗，氮气吹干，置于烘箱中将光纤表面的-OH固化；取出，常温下浸泡于10％氨丙基三甲氧基硅烷的甲醇溶液中6-12h，此时光纤表面被-NH2修饰，取出，用甲醇清洗、氮气吹干，置于烘箱中将光纤表面的-NH2固化；b) Functional modification: Soak the optical fiber sensing area obtained in step a) in piranha lotion, take out the optical fiber surface after being modified with -OH, wash it with deionized water, dry it with nitrogen, and place it in an oven to dry the optical fiber surface -OH solidification; take it out, soak it in methanol solution of 10% aminopropyltrimethoxysilane at room temperature for 6-12h, at this time the surface of the optical fiber is modified by -NH 2 , take it out, wash it with methanol, dry it with nitrogen, and put it in Curing -NH 2 on the surface of the optical fiber in an oven;
c)金种连接：将步骤b)获得的表面带有牢固的-NH2基团的光纤传感区域浸泡于金种溶液中8-12h，取出，去离子水清洗，氮气吹干；c) Gold seed connection: immerse the optical fiber sensing area with a firm -NH2 group on the surface obtained in step b) in the gold seed solution for 8-12h, take it out, wash it with deionized water, and dry it with nitrogen;
d)镀膜：将步骤c)获得的带有金种的光纤传感区域浸泡于镀膜液中，于振荡器中镀膜反应5-8min；d) Coating: soak the optical fiber sensing area with gold species obtained in step c) in the coating solution, and react in the oscillator for 5-8 minutes;
e)端面封银：采用银镜反应，得到终端反射式SPR传感器。e) Silver sealing on the end surface: adopt the silver mirror reaction to obtain the terminal reflective SPR sensor.
所述步骤a)中，光纤小段终端长度0.5-2cm为传感区域。In the step a), the length of the terminal end of the small optical fiber segment is 0.5-2 cm as the sensing area.
所述步骤a)中，传感区域浸泡于85℃的浓硫酸中。In the step a), the sensing area is soaked in concentrated sulfuric acid at 85°C.
所述步骤b)中，食人鱼洗液为体积比为7:3的浓硫酸与双氧水的混合液。In the step b), the piranha lotion is a mixture of concentrated sulfuric acid and hydrogen peroxide with a volume ratio of 7:3.
所述步骤b)中，光纤浸泡于食人鱼洗液温度为70-90℃。In the step b), the optical fiber is soaked in the piranha washing solution at a temperature of 70-90°C.
所述步骤d)中，镀膜液为0.1％HAuCl4与0.4mMNH2OH·HCl的混合液。In the step d), the coating solution is a mixed solution of 0.1% HAuCl 4 and 0.4mM NH 2 OH·HCl.
所述步骤d)中，振荡器转速需为100rpm。In the step d), the oscillator speed needs to be 100rpm.
本发明的方法也可以用来制备棱镜型SPR传感器、在线传输式等各种传输模式的SPR传感器、U型等各种形状的SPR传感器以及其它金膜传感器。The method of the present invention can also be used to prepare prism-type SPR sensors, SPR sensors of various transmission modes such as on-line transmission type, SPR sensors of various shapes such as U-shaped and other gold film sensors.
与现有SPR传感器制备方法相比，本发明的优点在于：1)本发明的制备SPR传感器方法，不使用物理蒸发或喷溅法中涉及的大型且昂贵的设备，所以该方法方便简单，成本低。Compared with the existing SPR sensor preparation method, the advantages of the present invention are: 1) The preparation SPR sensor method of the present invention does not use large and expensive equipment involved in physical evaporation or sputtering, so the method is convenient and simple, and the cost is low. Low.
2)本发明的金种生长法制备光纤型SPR传感器，解决了物理镀膜中必须使用转动装置以保证光纤柱面膜厚均匀的缺陷。2) The optical fiber type SPR sensor is prepared by the gold seed growth method of the present invention, which solves the defect that a rotating device must be used in the physical coating to ensure uniform thickness of the optical fiber cylindrical film.
3)本发明方法制备的光纤SPR传感器，对周围环境折射率有明显感应(见附图3)，灵敏度高，分别在折射率为1.333-1.359与1.359-1.386范围内，灵敏度为2054nm/RIU与3980nm/RIU，见附图4。3) The optical fiber SPR sensor prepared by the method of the present invention has obvious induction to the refractive index of the surrounding environment (see accompanying drawing 3), and the sensitivity is high, respectively in the scope of the refractive index of 1.333-1.359 and 1.359-1.386, and the sensitivity is 2054nm/RIU and 3980nm/RIU, see Figure 4.
附图说明Description of drawings
图1金种生长法制备终端反射式光纤表面等离子共振传感器流程图。Fig. 1 Flow chart of preparation of terminal reflective optical fiber surface plasmon resonance sensor by gold seed growth method.
图2金种生长法制备的终端反射式光纤SPR传感器实物照片。Fig. 2 The photo of the terminal reflective optical fiber SPR sensor prepared by the gold seed growth method.
图3金种生长法制备的光纤SPR传感器在不同折射率溶液中的反射光谱。Fig. 3 Reflection spectra of optical fiber SPR sensor prepared by gold seed growth method in different refractive index solutions.
图4金种生长法制备的光纤SPR传感器灵敏度考察。Fig. 4 Sensitivity investigation of optical fiber SPR sensor prepared by gold seed growth method.
具体实施方式Detailed ways
实施例1Example 1
将光纤进行去除聚合物、去除包覆层预处理后，分别用去离子水与乙醇清洗，氮气吹干后，浸泡于70-90℃的食人鱼洗液(体积比为7:3的浓硫酸与双氧水的混合液)中30min，取出后用去离子水清洗，氮气吹干，得到-OH修饰的光纤表面，将其置于100℃烘箱中1h，将光纤表面的-OH固化；取出，将带有-OH的光纤常温下浸泡于10％氨丙基三甲氧基硅烷(APTMS)的甲醇溶液中8h，取出后用甲醇清洗，氮气吹干，得到-NH2修饰的光纤表面，将其置于110℃烘箱中1h，将光纤表面的-NH2固化。采用传统的柠檬酸钠还原氯金酸法制备粒径约2.5nm的金种，将上述-NH2化后的光纤置于金种中8h-10h，取出后用去离子水清洗，氮气吹干备用。配制镀膜液(0.1％HAuCl4与0.4mMNH2OH·HCl的混合液)，将带有金种的光纤浸泡于镀膜液中，于振荡器中100rpm反应7min，光纤表面形成一层致密的金膜。对金膜进行端面封银，制得基于金种生长法制备的终端反射式光纤SPR传感器(见附图2)。After the optical fiber is pretreated to remove the polymer and the cladding layer, it is cleaned with deionized water and ethanol respectively, dried with nitrogen, and soaked in piranha washing solution at 70-90°C (concentrated sulfuric acid with a volume ratio of 7:3 mixed solution with hydrogen peroxide) for 30 minutes, take it out, wash it with deionized water, and blow it dry with nitrogen to get the surface of the optical fiber modified by -OH, put it in an oven at 100°C for 1 hour, and cure the -OH on the surface of the optical fiber; take it out, and put The optical fiber with -OH was soaked in a methanol solution of 10% aminopropyltrimethoxysilane (APTMS) at room temperature for 8 hours, cleaned with methanol after taking it out, and dried with nitrogen to obtain -NH2 Modified optical fiber surface, which was placed In an oven at 110°C for 1 h, the -NH 2 on the fiber surface was cured. Prepare gold seeds with a particle size of about 2.5nm by using the traditional method of reducing chloroauric acid with sodium citrate. Put the optical fiber after the above -NH 2 into the gold seeds for 8h-10h, take it out, wash it with deionized water, and dry it with nitrogen gas spare. Prepare the coating solution (a mixture of 0.1% HAuCl 4 and 0.4mMNH 2 OH·HCl), soak the optical fiber with gold seeds in the coating solution, and react in the oscillator at 100rpm for 7min, and a dense gold film is formed on the surface of the optical fiber . The end surface of the gold film was sealed with silver to obtain a terminal reflective optical fiber SPR sensor based on the gold seed growth method (see Figure 2).
将上述基于金种生长法制得的光纤SPR传感器通过SMA905等接头安装到SPR谱仪测控系统。设定积分时间、平均次数、平滑度，待信号稳定后保存暗光谱；打开光源，待信号稳定后保存参考光谱；将界面调节至反射率模式，将制备的传感器浸入水中，待信号稳定后叠加活动光谱，得到传感器在水中的SPR反射谱图，同样，依次将制得的传感器浸入乙腈、丙酮、乙醇、己烷、正丙醇溶液中，得到传感器在上述几种溶液中的SPR反射谱图。Origin软件作图，得到基于金种生长法制备的SPR传感器在以上不同折射率的溶液中的反射谱图(见附图3)；通过计算，得到基于金种生长法制备的SPR传感器分别在1.333-1.359与1.359-1.386的折射率范围内的灵敏度为2054nm/RIU与3980nm/RIU(见附图4)。Install the optical fiber SPR sensor based on the above-mentioned gold seed growth method to the SPR spectrometer measurement and control system through SMA905 and other connectors. Set the integration time, average times, and smoothness, and save the dark spectrum after the signal is stable; turn on the light source, and save the reference spectrum after the signal is stable; adjust the interface to reflectivity mode, immerse the prepared sensor in water, and superimpose after the signal is stable Active spectrum to obtain the SPR reflection spectrum of the sensor in water. Similarly, the prepared sensor is immersed in acetonitrile, acetone, ethanol, hexane, and n-propanol solutions in turn to obtain the SPR reflection spectrum of the sensor in the above solutions . Origin software plots, obtains the reflectance spectrum (see accompanying drawing 3) of the SPR sensor prepared based on the gold seed growth method in the solution of the above different refractive indices; by calculation, obtains the SPR sensor prepared based on the gold seed growth method at 1.333 The sensitivities in the refractive index ranges of -1.359 and 1.359-1.386 are 2054nm/RIU and 3980nm/RIU (see Figure 4).
实施例2Example 2
将光纤进行去除聚合物、去除包覆层预处理后，分别用去离子水与乙醇清洗，氮气吹干后，浸泡于70-90℃的食人鱼洗液(体积比为7:3的浓硫酸与双氧水的混合液)中30min，取出后用去离子水清洗，氮气吹干，得到-OH修饰的光纤表面，将其置于100℃烘箱中1h，将光纤表面的-OH固化；取出，将带有-OH的光纤常温下浸泡于10％氨丙基三甲氧基硅烷(APTMS)的甲醇溶液中6h，取出后用甲醇清洗，氮气吹干，得到-NH2修饰的光纤表面，将其置于110℃烘箱中1h，将光纤表面的-NH2固化。采用传统的柠檬酸钠还原氯金酸法制备粒径约2.5nm的金种，将上述-NH2化后的光纤置于金种中8h，取出后用去离子水清洗，氮气吹干备用。配制镀膜液(0.1％HAuCl4与0.4mMNH2OH·HCl的混合液)，将带有金种的光纤浸泡于镀膜液中，于振荡器中100rpm分别反应5min、6min、7min和8min。对金膜进行端面封银，制得基于金种生长法制备的不同镀膜时间下的终端反射式光纤SPR传感器。After the optical fiber is pretreated to remove the polymer and the cladding layer, it is cleaned with deionized water and ethanol respectively, dried with nitrogen, and soaked in piranha washing solution at 70-90°C (concentrated sulfuric acid with a volume ratio of 7:3 mixed solution with hydrogen peroxide) for 30 minutes, take it out, wash it with deionized water, and blow it dry with nitrogen to get the surface of the optical fiber modified by -OH, put it in an oven at 100°C for 1 hour, and cure the -OH on the surface of the optical fiber; take it out, and put The optical fiber with -OH was soaked in a methanol solution of 10% aminopropyltrimethoxysilane (APTMS) at room temperature for 6 hours, cleaned with methanol after taking it out, and dried with nitrogen to obtain -NH 2 Modified optical fiber surface, which was placed In an oven at 110°C for 1 h, the -NH 2 on the fiber surface was cured. Gold seeds with a particle size of about 2.5 nm were prepared by the traditional sodium citrate reduction method of chloroauric acid, and the above-NH 2 optical fiber was placed in the gold seeds for 8 hours, cleaned with deionized water after removal, and dried with nitrogen gas for later use. Prepare coating solution (a mixture of 0.1% HAuCl 4 and 0.4mM NH 2 OH·HCl), soak the optical fiber with gold species in the coating solution, and react in an oscillator at 100 rpm for 5 min, 6 min, 7 min and 8 min respectively. The end surface of the gold film was sealed with silver, and the terminal reflective optical fiber SPR sensor with different coating time was prepared based on the gold seed growth method.
按照实施例1中的测定方法，分别测定镀膜时间为5min、6min、7min和8min的传感器在水中的SPR反射谱图，通过origin软件作图，并比较，得知：镀膜时间为7min时，得到的传感器SPR信号最佳。According to the measurement method in Example 1, measure the SPR reflectance spectrum of the sensor in water that the coating time is 5min, 6min, 7min and 8min respectively, draw the graph by origin software, and compare, know: when the coating time is 7min, get The sensor SPR signal is the best.
本发明公开和提出的一种基于金种生长的终端反射式光纤表面等离子共振传感器制备方法，本领域技术人员可通过借鉴本文内容，适当改变条件和工艺路线等环节实现，尽管本发明的方法和制备技术已通过较佳实施例子进行了描述，相关技术人员明显能在不脱离本发明内容、精神和范围内对本文所述的方法和技术路线进行改动或重新组合，来实现最终的制备技术。特别需要指出的是，所有相类似的替换和改动对本领域技术人员来说是显而易见的，他们都被视为包括在本发明精神、范围和内容中。The present invention discloses and proposes a method for preparing a terminal reflective optical fiber surface plasmon resonance sensor based on the growth of gold seeds. Those skilled in the art can learn from the content of this article and appropriately change the conditions and process routes. Although the method of the present invention and The preparation technology has been described through preferred implementation examples, and it is obvious that those skilled in the art can modify or recombine the methods and technical routes described herein without departing from the content, spirit and scope of the present invention to realize the final preparation technology. In particular, it should be pointed out that all similar substitutions and modifications will be obvious to those skilled in the art, and they are all considered to be included in the spirit, scope and content of the present invention.
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